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At least 289 records · Page 16
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

PROCESS-STRUCTURE-PROPERTY RELATIONSHIPS IN LASER POWDER BED FUSION PRODUCED 17-4 PH STEEL

Laser powder bed fusion (LPBF) is a metal additive manufacturing method that produces non-traditional microstructures as a result of the rapid solidification and thermal cycling inherent to the process. When using LPBF-produced material in application, these unique microstructures challenge the applicability of well developed mechanical property databases achieved by conventional heat treatments. For wider adoption of this technology, a more holistic understanding is necessary on how process attributes develop material structure, which dictate mechanical properties. This dissertation explores the process– structure–property relationships in LPBF 17-4 PH steel through systematic evaluation of atmospheric processing and heat treatment effects on microstructure and mechanical performance. Specimens were fabricated under controlled build environments, subjected to a range of solutionizing, homogenizing, and aging treatments, and characterized using optical microscopy, electron back scatter diffraction (EBSD), and X-ray diffraction (XRD) to quantify phase evolution. Tensile testing was performed to directly link heat treatment pathway and nitrogen absorption to mechanical performance. This work demonstrates where conventional heat treatment standards are applicable to LPBF 17-4 PH steel and where modifications are required. By directly correlating phase stability, nitrogen effects, and tensile response, this work provides practical guidelines for tailoring post-processing strategies. These findings underscore that successful application of LPBF 17-4 PH steel requires explicit consideration of both build environment and post-processing. By linking processing conditions to microstructure and performance, this work advances understanding of critical variables that govern reliability of additively manufactured precipitation-hardened stainless steels in demanding applications.

Brown, Benjamin [Kansas City National Security Cam↗
DOE OSTI2025

DEVELOPMENT OF INEXPENSIVE HIGH TEMPERATURE NITI-BASED SHAPE MEMORY ALLOYS FOR POWDER BED ADDITIVE MANUFACTURING

NiTi and NiTi-based Shape Memory Alloys (SMA) exhibit a reversible solid-state phase transformation from martensite to austenite driven by thermal energy. High temperature (Mf>100°C) SMAs are martensite at room temperature and can be fabricated into solid-state actuators that return to a pre-programmed shape against a designed load after heating to transformation threshold. Reactive as-fabricated additively manufactured parts (4-D printing) is the current state of the art in manufacturing of SMAs but requires compositions compliant to rapid solidification. Existing actuator designs are developed from commercially available, highly investigated material compositions. However, existing high temperature high performance (high actuation strain, low thermal hysteresis) shape memory alloys contain significant (>10% at.) portions of high-cost Platinum Group Metals (PGMs). It is of significant scientific interest to investigate material compositions that are peer performing or superior to PGMs whose constituent elements represent a significant cost savings. Shape memory alloy properties vary significantly with small (0.1% at.) compositional changes making robust investigative sample sets very large. Computational material design can be deployed to shrink the compositional space of possible alloy combinations and reduce the experimental load in material discovery. Investigating shape memory effect (SME) and validating process additive process parameters for a single novel composition is cost intensive in both time and consumed materials. Additionally, sub-optimal processing, oxygen, or solidification rate sensitivity could render additively manufacturing specimens without micro, macro cracks, or significant chemical variance impossible. Unfortunately, such failure susceptibility cannot be simulated. Therefore, a research pathway to validate novel shape memory alloy compositions for powder bed fusion additive manufacturing without the need for powdered feedstock is also proposed. This research investigates novel high temperature shape memory alloys for actuators without platinum group alloying elements to discover one that could be commercially viable as an additive manufacturing feedstock.

Sundermann, Tayler↗
DOE OSTI2025

Novel Synthesis and Characterization of Uranium-Zirconium Carbonitride by Direct Casting

UZrCN has exhibited thermophysical properties beneficial to high temperature reactor applications such as nuclear thermal rockets. The present work investigates a novel liquid phase synthesis method involving the admission of nitrogen gas during arc melting of uranium, zirconium, and carbon. Initial microstructural examinations using SEM indicated that the samples remain heterogenous with zirconium-rich cores in a uranium-rich matrix. Heterogeneity resulted from large differences in melting temperature of the major constituents and rapid solidification. Additional EDS, combustion analysis, and inert gas fusion analysis proved that the core regions have both uranium and zirconium and establish that carbon and nitrogen are retained during the fabrication process. XRD clarifies that the light elements did not form compounds with the uranium matrix but rather incorporated into the core region forming a sub-stoichiometric UZrCN. Heat treatment performed on equimolar U-Zr-C resulted in an increase in the homogenous phase present with an XRD pattern reflecting a ternary UZrCN despite small amounts of segregation in the final button.

36 - MATERIALS SCIENCE↗
DOE OSTI2025

On Uranium-Zirconium Carbonitride Formation by Direct Casting - A Novel Synthesis Study

UZrCN has exhibited thermophysical properties beneficial to high temperature reactor applications such as nuclear thermal rockets. The present work investigates a novel liquid phase synthesis method involving the admission of nitrogen gas during arc melting of uranium, zirconium, and carbon. Initial microstructural examinations using SEM indicated that the samples remain heterogenous with zirconium-rich cores in a uranium-rich matrix. Heterogeneity resulted from large differences in melting temperature of the major constituents and rapid solidification. Additional EDS, combustion analysis, and inert gas fusion analysis proved that the core regions have both uranium and zirconium and establish that carbon and nitrogen are retained during the fabrication process. XRD clarifies that the light elements did not form compounds with the uranium matrix but rather incorporated into the core region forming a sub-stoichiometric UZrCN. Heat treatment performed on equimolar U-Zr-C resulted in an increase in the homogenous phase present with an XRD pattern reflecting a ternary UZrCN despite small amounts of segregation in the final button.

36 - MATERIALS SCIENCE↗
NASA NTRS1984

Orientation and Morphology Effects in Rapid Silicon Sheet Solidification

Radial growth anisotropies and equilibrium forms of point nucleated, dislocation free silicon sheets spreading horizontally on the free surface of a silicon melt were measured for (100), (110), (111), and (112) sheet planes. The growth process was recorded. Qualitative Wulff surface free energy polar plots were deduced from the equilibrium shapes for each sheet plane. Predicted geometries for the tip shape of unidirectional, dislocation free, horizontally grown sheets growing in various directions within the planes were analyzed. Polycrystalline sheets and dendrite propagation were analyzed. For dendrites, growth rates on the order of 2.5 m/min and growth rate anisotropies of 25 are measured.

Ciszek, T. F.↗
DOE OSTI2025

Isothermal solidification for high-entropy alloy synthesis

Kinetically trapping the high-temperature states through rapid cooling solidification is widely used for the synthesis of high-entropy alloys (HEAs), especially those with intrinsically immiscible elemental combinations. However, strategies need to be developed to overcome the fundamental limitations of rapid cooling solidification in controlling the crystallinity, structure and morphology of HEAs. Here, in this study, we introduce an isothermal solidification strategy for the synthesis of HEAs by rapidly altering the metal alloy composition through liquid–liquid interface reactions at low temperatures, for example, from 25 °C to 80 °C. We use gallium (Ga)-based metal as the sacrificial reagent and mixing medium. By directing the reactions to the interfaces between the Ga-based liquid metal and an aqueous metal ion solution, the foreign metal ions can be reduced at the interfaces and incorporated into the liquid metal quickly. HEAs with various crystallinity (single crystal, mesocrystal, polycrystal and amorphous), morphology (zero, two and three dimensions) and compositions can be achieved through the isothermal solidification. Ga can be completely consumed, resulting in Ga-free HEAs. If desired, Ga can be one of the metal elements in the final products. In situ liquid phase transmission electron microscopy (TEM) studies and theoretical analysis show the isothermal solidification mechanisms. Our direct observations show the enhanced mixing of liquid metal elements and the solidification process with fluctuating nucleation dynamics. The isothermal solidification marks a powerful strategy for HEA synthesis through an unexplored pathway of kinetically trapping the high-entropy states.

Zhang, Qiubo [Lawrence Berkeley National Laborator↗
DOE OSTI2023

Microstructural Pattern Formation during Far-from-Equilibrium Alloy Solidification

We introduce a new phase-field formulation of rapid alloy solidification that quantitatively in- corporates non-equilibrium effects at the solid-liquid interface over a very wide range of interface velocities. Simulations identify a new dynamical instability of dendrite tip growth driven by solute trapping at velocities approaching the absolute stability limit. They also reproduce the formation of the widely observed banded microstructures, revealing how this instability triggers transitions between dendritic and microsegregation-free solidification. Predicted band spacings agree quantita- tively with observations in rapidly solidified Al-Cu thin films.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Mechanical Properties of Solidifying Assemblies of Nanoparticle Surfactants at the Oil–Water Interface

The effect of polymer surfactant structure and concentration on the self-assembly, mechanical properties, and solidification of nanoparticle surfactants (NPSs) at the oil-water interface was studied. The surface tension of the oil-water interface was found to depend strongly on the choice of the polymer surfactant used to assemble the NPSs, with polymer surfactants bearing multiple polar groups being the most effective at reducing interfacial tension and driving the NPS assembly. By contrast, only small variations in the shear modulus of the system were observed, suggesting that it is determined largely by particle density. In the presence of polymer surfactants bearing multiple functional groups, NPS assemblies on pendant drop surfaces were observed to spontaneously solidify above a critical polymer surfactant concentration. Interfacial solidification accelerated rapidly as polymer surfactant concentration was increased. On long timescales after solidification, pendant drop interfaces were observed to spontaneously wrinkle at sufficiently low surface tensions (approximately 5 mN m -1 ). Interfacial shear rheology of the NPS assemblies was elastic-dominated, with the shear modulus ranging from 0.1 to 1 N m -1 , comparable to values obtained for nanoparticle monolayers elsewhere. Finally, our work paves the way for the development of designer, multicomponent oil-water interfaces with well-defined mechanical, structural, and functional properties.

36 MATERIALS SCIENCE↗
NASA NTRS1984

Solidification of undercooled metals

The present investigation is concerned with the subject of undercooling (i.e., supercooling) in the case of metal alloys, taking into account the effects of undercooling on microstructure and microsegregation in alloys which solidify in a crystalline manner. Techniques for obtaining a large degree of undercooling are discussed. These techniques make it possible to eliminate heterogeneous nucleants from the melt and to remove container nucleation effects. The nucleation behavior of small metal droplets is considered along with the formation of a dispersion of fine droplets in a suitable inert medium, the mixing of fine metal powders with glass powder, and the levitation melting technique. Attention is given to solidification with rapid interface velocity, aspects of dendritic morphology, and thermal measurements during solidification of undercooled droplets.

Flemings, M. C.↗
DOE OSTI2017

Comparative study of solute trapping and Gibbs free energy changes at the phase interface during alloy solidification under local nonequilibrium conditions

An analytical model has been developed to describe the influence of solute trapping during rapid alloy solidification on the components of the Gibbs free energy change at the phase interface with emphasis on the solute drag energy. For relatively low interface velocity V < V{sub D}, where V{sub D} is the characteristic diffusion velocity, all the components, namely mixing part, local nonequilibrium part, and solute drag, significantly depend on solute diffusion and partitioning. When V ≥ V{sub D}, the local nonequilibrium effects lead to a sharp transition to diffusionless solidification. The transition is accompanied by complete solute trapping and vanishing solute drag energy, i.e. partitionless and “dragless” solidification.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS2018

Preparation of Thick NI/AL Reactive Multilayer Films and Prospective Use for Self-Powered Brazing of TI-6AL-4V

In this study we demonstrate a new method for depositing thick reactive multilayer films (RMFs) (thickness > 14 µm) by using Ti interlayer integration and substrate preheating during fabrication. These two adjustments are designed to alleviate internal planar stresses that cause delamination between deposited layers and peeling off the substrate. Decreasing the distance between Ti interlayers helps to eliminate delamination between deposited layers. Through high speed camera measurements, the reaction propagation speed of an RMF sample with preheating is 42% slower than the same RMF that was not preheated, indicating a slower heat release rate. The preliminary experiments on brazing Ti-6Al-4V coated with BAlSi-4 brazing material revealed dendritic structure branching out from the RMF surface into the brazing material. The dendrite structures most likely form because of rapid melting and solidification of the brazing material. However, this rapid melting and solidification cycle does not appear to occur uniformly across the BAlSi-4RMF interface which is linked to its low bonding strength. When the Ti-6Al-4V substrate is heated to 150 °C prior to ignition, the strength increases to 0.47 MPa when the total RMF thickness is 84 µm and 15 MPa of pressure is applied.

Cheng, Jinquan↗
DOE OSTI2024

Grain structure and texture selection regimes in metal powder bed fusion

Additive manufacturing (AM) offers opportunities to produce complex part geometries not possible with conventional processing and in some cases even improve part performance. However, adoption has been slowed by difficulties assessing microstructure variability and there is no straightforward approach to relate processing to grain structure characteristics. In this study, datasets from AdditiveFOAM heat transport simulations of laser powder bed fusion (LPBF) are used to drive ExaCA simulations of grain structure. The GPU utilization of ExaCA and an algorithmic update for modeling melt pool overlap region solidification enabled rapid and parallel simulation across a wider range of process conditions than previously explored with cellular automata-based solidification models. A texture selection angle $θ_s$ is defined based on melt pool overlap geometry, and the range of $θ_s$ over which a commonly observed texture transition occurs in characterized AM builds was well-reproduced by ExaCA simulations over a wide range of melt pool shape, hatch spacing, and layer height. ExaCA simulations with 90 degree rotation of the scan direction on every other layer reproduced a number of trends from the AM literature including grain refinement, the dominance of layers with larger melt pools on the final grain structure, and the weakening or strengthening of texture depending on odd and even layer melt pool overlap geometry. EBSD data from a benchmark AM part is used to validate the simulated mechanism of a layer rotation-induced texture strengthening effect. Importantly, these results expand the understanding of the mechanisms for texture selection in alloys with cubic crystal symmetry and offer an approach to easily evaluate processing conditions. With this new understanding, these modeling tools will enable anticipation of previously unexpected variations in grain structure and target specific microstructures and properties.

36 MATERIALS SCIENCE↗
NASA NTRS1985

Variable-Temperature-Gradient Device for Solidification Research

Device for research in solidification and crystal growth allows crystallization of melt observed as occurs. Temperature gradient across melt specimen increased or decreased rapidly while solidification front proceeds at constant speed across sample. Device moves sample at same speed, thereby holding position of liquid/solid interface stationary within field of optical microscope. Device, variabletemperature-gradient microscope stage, used to study crystal growth at constant rate while thermal driving force is varied.

Kaukler, W. F.↗
NASA NTRS1992

FNAS modify matric and transparent experiments

Monotectic alloy materials are created by rapid melt/rapid solidification processing on the NASA KC-135. Separation of the uniform liquid into two liquids may occur by either of two processes; spinodal decomposition or nucleation followed by growth. In the first case, the liquid is unstable to composition waves, which form and grow, giving liquids of two different compositions. In the latter process discrete particles of the second liquid phase form via thermal fluctuations and then grow by diffusion. The two processes are very different, with the determining process being dictated by temperature, composition, and thermodynamic characteristics of the alloy. The first two quantities are process variables, while the third is determined by electronic interactions between the atoms in the alloy. In either case the initial alloy decomposition is followed by coarsening, resulting in growth of the particle size at nearly constant volume fraction. In particular, reduced gravity experiments on monotectic solutions have shown a number of interesting results in the KC-135. Monotectic solutions exhibit a miscibility gap in the liquid state, and consequently, gravity driven forces can dominate the solidification parameters at 1 g. In reduced gravity however, the distribution of the phases is different, resulting in new and interesting microstructures. The Rapid Melt/Rapid Quench Furnace allows one to melt a sample and resolidify it in one parabola of the KC-135's flight path, thus eliminating any accumulative influence of multiple parabolas to affect the microstructure of the material.

Smith, Guy A.↗
DOE OSTI2025

Quantification and prediction of solidification textures under additive manufacturing conditions

Crystallographic textures are a major determinant of the macroscale anisotropic properties of polycrystalline metallic alloys produced in a wide range of additive manufacturing (AM) processes. Here, we introduce a statistical method that can accurately quantify the degree of orientational order of textures despite the large random fluctuations in the orientation of individual grains inherent in AM processes. The method, demonstrated for laser and resolidification of AlSi thin films, extends Z-scoring to a dynamical regime to assess the statistical significance of observed textures compared to randomly generated ones at different stages of solidification. We further show that, combined with phase-field modeling, this method can be used to infer fundamental anisotropic properties of the solid-liquid interface that are essential for texture prediction, and are compared here to the results of atomistic simulations. In addition, phase-field modeling reveals that, even at rapid AM solidification rates, the observed 〈110〉-dominated textures in the AlSi thin films are controlled predominantly by the anisotropy of the interface free-energy and sheds light on the physical mechanism of grain competition. These results significantly enhance both the existing tools for the quantification and prediction of AM crystallographic textures and our basic understanding of their formation.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Revisiting solidification microstructure selection maps in the frame of additive manufacturing

Understanding microstructural development in additive manufacturing under highly non-equilibrium cooling conditions and the consequent effects on mechanical properties of the final component is critical for accelerating industrial adoption of these manufacturing techniques. In this study, simple but effective theoretical solidification models are recalled to evaluate their ability to predict of microstructural features in additive manufacturing applications. As a case study, the resulting solidification microstructure selection maps are created to predict the stable growth modality and the columnar to equiaxed transition (CET) of an Al-10Si-0.5Mg alloy processed via Selective Laser Melting. The potential of this method in microstructural predictions for additively manufactured products, as well as outstanding challenges and limitations, are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of Sb substitution on crystal structure, texture and hard magnetic properties of melt-spun MnBi alloys

Melt-spun Mn 50 Bi 50-x Sb x alloys with x ≤ 5 were prepared at different solidification rates and characterized both in the as-spun state and after annealing. In the as-spun alloys, the Sb substitution leads to the formation of a metastable phase, similar to the binary "quenched high-temperature phase" but without the superstructure of the latter and exhibiting a different – increasing – temperature dependence of coercivity. The new nanocrystalline metastable phase is not only itself characterized by a high room-temperature coercivity (in excess of 20 kOe), but upon annealing it transforms into a high-coercivity (up to 13.5 kOe) "low-temperature" α phase. However, the advantage of obtaining a high coercivity without the otherwise required milling made possible by the Sb substitution is undermined by the absence of a local crystallographic texture in the melt-spun alloys. The best combination of the isotropic hard magnetic properties realized for the Mn 55 Bi 43.5 Sb 1.5 composition is a remanence of 35.5 emu/g and a coercivity of 8.1 kOe. The annealed Sb-free Mn 50 Bi 50 alloys did possess a local crystallographic alignment and, for high solidification rates, a moderate coercivity up to 5.6 kOe; however, they had an inadequate "rectangularity" in the demagnetization curve. The orthorhombic compound known as MnBi 0.9 Sb 0.1 and described earlier as antiferromagnetic was obtained in the annealed ribbons with x ≈ 5. The compound was found to order ferromagnetically between 200 K and ≈250 K and to exhibit a significant coercivity, 14.3 kOe at 50 K. Here, it is suggested that the MnBi 0.9 Sb 0.1 may actually be a Sb-stabilized "new phase" observed earlier as metastable in the Bi–MnBi eutectic alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructure and mechanical behavior of laser remelted amorphous Al-Ni-La welds

To explore the feasibility of using laser powder bed fusion systems to print bulk amorphous Al alloys, a single autogenous weld produced by laser remelting on a cast Al-5La-9Ni (at.%) alloy was studied for its microstructure and mechanical behavior. The solidification rates experienced by material within the welds were high enough to produce entirely amorphous regions within the welds. Welds were characterized using SEM, STEM, and APT and were found to contain Ni-rich amorphous clusters. Micropillar compression tests were used to assess mechanical properties of the welds and found that all of the amorphous regions exhibited yield strengths around 1 GPa. In conclusion, these results are discussed in the context of diffusivity of Ni and rare earth elements in liquid, glass forming ability, thermodynamic driving force for phase formation during solidification, free volume concentrations in bulk metallic glasses, and cluster-related softening.

APT↗